US6946030B2 - Method for the production of a silica glass crucible with crystalline regions from a porous silica glass green body - Google Patents

Method for the production of a silica glass crucible with crystalline regions from a porous silica glass green body Download PDF

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US6946030B2
US6946030B2 US10/292,059 US29205902A US6946030B2 US 6946030 B2 US6946030 B2 US 6946030B2 US 29205902 A US29205902 A US 29205902A US 6946030 B2 US6946030 B2 US 6946030B2
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green body
crucible
silica glass
silica
silicon
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US20030159648A1 (en
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Fritz Schwertfeger
Holger Szillat
Christoph Frey
Ulrich Lambert
Axel Frauenknecht
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Wacker Chemie AG
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Wacker Chemie AG
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
    • C30B35/002—Crucibles or containers
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
    • C03B19/066—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction for the production of quartz or fused silica articles
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B20/00—Processes specially adapted for the production of quartz or fused silica articles, not otherwise provided for
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
    • C03B32/02—Thermal crystallisation, e.g. for crystallising glass bodies into glass-ceramic articles
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/10—Crucibles or containers for supporting the melt
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S65/00—Glass manufacturing
    • Y10S65/08—Quartz
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
    • Y10T117/10—Apparatus
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
    • Y10T117/10—Apparatus
    • Y10T117/1024—Apparatus for crystallization from liquid or supercritical state
    • Y10T117/1032—Seed pulling
    • Y10T117/1052—Seed pulling including a sectioned crucible [e.g., double crucible, baffle]

Definitions

  • the invention relates to a method for the production of a silica glass crucible with crystalline regions from a porous silica glass green body, and to the use of the method for pulling Si single crystals according to the Czochralski method (“CZ method”).
  • CZ method Czochralski method
  • quartz glass crucibles which are melted from crystalline SiO 2 particles (for example quartz sand) in a melting process, generally in an arc discharge.
  • crystalline SiO 2 particles for example quartz sand
  • a closed, amorphous, vitrified inner layer and a fully vitrified outer body with low porosity are formed. It is desirable that the inner layer contain the fewest possible amount of bubbles, and when present, in the smallest possible size.
  • Impurities in the inner surface of the crucible are a limiting factor for crucible life within which it is possible to produce monocrystalline material.
  • the crystalline quartz layer then created in the CZ method reaches only a thickness of less than 1 mm when coating the inside of the crucible, and less than 2 mm when coating the outside of the crucible. This means that the increase in stability of the crucible when coating the outside of the crucible is unduly limited.
  • the very thin crystalline layer that is formed in the CZ method leads to mechanical stresses between the crystalline and amorphous regions of the quartz glass crucible. These are due to the differing thermal expansion coefficients and the differing mechanical stabilities of the amorphous and crystalline modifications of the crucible material as a function of temperature. As a result of these stresses, quartz particles may be displaced from the inner surface of the crucible and, via the Si melt, reach the growing crystal where they induce undesired dislocations.
  • the bubbles present in the amorphous starting material can grow at an unreduced rate during the CZ method and, when displaced, likewise contribute to the emission of quartz glass particles into the Si melt.
  • FIG. 1 shows a photographic image of a cross section of a silica glass crucible, which was formed by using the method according to Example 2.
  • the cristobalite layers A which include a core of amorphous quartz glass B, can be seen clearly here together with a silicon layer C in the interior of the crucible.
  • FIG. 2 shows a comparison of the Oi content in relation to the crystal length L of crystallites, which were produced by using standard quartz crucibles (S), and a crucible produced according to the invention by using Example 2 (N).
  • FIG. 3 shows a comparison of the Oi precipitation of crystals, which were produced by using standard quartz crucibles S 1 and S 2 , with a crucible N produced according to the invention by using Example 2.
  • the present invention pertains to a method wherein a) a porous amorphous silica glass green body, which is infiltrated with at least one substance that promotes crystallization of a silica glass crucible, is produced, b) the infiltrated silica glass green body is dried, c) filled with a metal or semimetal and d) heated for a period of from 1 h to 1000 h to a temperature of from 900 to 2000° C.
  • a crystalline phase preferably cristobalite, is formed in situ in the silica glass crucible during or after the melting of the metal or semimetal.
  • a single crystal from the metal or semimetal melted in the crucible for example an Si single crystal according to the CZ method, the disadvantages known from the prior art do not arise.
  • a silica glass green body is intended to mean a porous amorphous shaped body with a crucible shape produced from amorphous SiO 2 particles (silica glass) by conventional shaping steps.
  • a silica glass crucible is intended to mean a shaped body with a crucible shape produced by sintering and/or melting a silica glass green body.
  • Silica glass green bodies suitable as starting materials for the method according to the invention are known. They are described, for example, in the U.S. Pat. No. 5,053,359 or German published application DE-A-19943103.
  • the silica glass green body is, for example as described in DE-A-19943103, fully or partially supplemented with a compound that promotes or causes crystallization of SiO 2 , preferably formation of cristobalite. All compounds known to one skilled in the art are suitable. Non-limiting examples include the compounds described in EP 0753605, U.S. Pat. No. 5,053,359 and GB 1428788. It is to be expected that further suitable compounds will be discovered in the future.
  • a “crystallization inducing” compound is preferably selected from among barium, aluminum and boron compounds, and mixtures thereof. Ba(OH) 2 , barium oxide, barium carbonate or aluminum oxide are particularly preferred. Ba(OH) 2 , barium oxide or barium carbonate are more particularly preferred.
  • the crystallization-inducing compound may be added to the starting material for the production of the silica glass green body before and/or after the crucible shaping. This may be done using methods known in the prior art. If the addition is to take place after the crucible shaping, addition generally involves application to and/or penetration into the surface of the silica glass green body. This may be done both before drying and after drying the silica glass green body.
  • the addition of the crystallization-inducing compound may take place in a liquid and/or a solid form. If the compounds are added in liquid form, solutions thereof are generally used. All solvents in which the respective substance dissolves at a sufficient concentration are in principle suitable as solvents in this case. Water is the preferred solvent.
  • the concentration of the crystallization-inducing compounds in the solution is preferably between 0.001 and 100% by weight, more preferably between 0.001 and 10% by weight, and most preferably between 0.001 and 1% by weight.
  • the solutions may be applied one or more times in a controlled manner, for example by spraying, immersion or impregnation. Since open-pored silica glass green bodies are involved, the solution in this case penetrates with the aid of capillary forces into the pores in the silica glass green body, where it preferably wets the surface of pores. Single or repeated controlled electrophoretic deposition of the crystallization-inducing substances dissolved in solvent into the pores of the silica glass green body is also possible.
  • the silica glass green body is subsequently dried.
  • it may also be dried between the individual application steps. Drying is generally performed at temperatures between room temperature and the boiling point of the solvent that is used. In the case of water as the solvent, drying preferably takes place between 40° C. and 100° C., more preferably between 70° C. and 95° C.
  • drying may also be performed under vacuum.
  • the concentration of the crystallization-inducing compounds in the pore surfaces may furthermore be adjusted as desired.
  • a crucible wall having a crystallization-inducing compound-containing inner and/or outer layer with a respectively desired thickness, or a crystallization-inducing compound-containing layer lying fully in the interior of the crucible wall, or a silica glass green body fully permeated with the crystallization-inducing compounds.
  • the compounds are used in the solid form, then they are preferably added directly to the SiO 2 -containing dispersion from which a crucible-shaped silica glass green body will be formed.
  • the compounds may be used in all particle sizes and shapes, although it is preferable to employ particles of the order of magnitude of the SiO 2 particles employed for the dispersion. Preferably, all particles in the dispersion are distributed as homogeneously as possible.
  • the production of the dispersion as well as the addition and distribution of the particulate compounds to and within the dispersion follows conventional methods known to those skilled in the art.
  • the production of the shaped body from such dispersions likewise follows customary methods known to the skilled artisan, for example as disclosed in DE 19943103.
  • crystallization-inducing compounds added in solid form are distributed not only on the surface of the pores of the dried silica glass green body, but also between the SiO 2 particles that form the crucible. Electrophoretic deposition of the compound particles into the pores of a silica glass green body is also possible.
  • crystalline SiO 2 particles As described in U.S. Pat. No. 4,018,615, it is also possible to induce crystallization by adding crystalline SiO 2 particles to the dispersion and/or to the porous silica glass green body.
  • the crystalline SiO 2 particles preferably have the same particle sizes as the amorphous particles that form the silica glass green body.
  • a crystallization-inducing compound-containing silica glass green body is then preferably subjected to a heat treatment (partial sintering), preferably at temperatures between 500° C. and 1300° C., more preferably between 800° C. and 1100° C. Duration of sintering is preferably from 1 to 180 min., more preferably from 1 to 60 min. During this process, the grain boundaries merge with one another, so-called grain necks being formed, which leads to increased mechanical stability of the silica glass green body. During this heat treatment, however, an open porosity of the silica glass green body must be preserved.
  • a silica glass green body produced in this manner is then filled with one or more metals or semimetals.
  • the metals or semimetals are in this case preferably present in the form of lumps and/or granules and/or powder. In principle, it is possible to use all known metals or semimetals, or mixtures thereof.
  • poly- and/or monocrystalline silicon, more preferably high-purity poly- or monocrystalline silicon, or mixtures thereof, are used.
  • the silica glass green body filled with a metal or semimetal is heated, preferably over a period of from 10 to 1500 minutes, until a temperature of between 1000 and 1600° C., more preferably between 1300 and 1500° C., prevails in the metal melt.
  • the heating leads, before, during and after melting of the metal, to crystallization in the regions in the silica glass crucible which are supplemented with substances that promote crystallization. Cristobalite structures are preferably created during the crystallization.
  • the concentration of crystalline SiO 2 can advantageously be controlled though the nature and concentration of the substances that promote crystallization, as well as through the temperature and the duration of the heating. Through suitable selection of the melt conditions for the polycrystalline silicon, it is possible to influence the sintering and crystallization behavior of the silica glass crucible. For a silica glass green body produced using the especially preferred concentration of the compound that promotes crystallization, i.e. from 0.01 to 100 ⁇ g of compound per g of SiO 2 , it is particularly preferred to heat a silica glass green body over a period of from 40 to 800 minutes, reaching a temperature of 1300° C.
  • liquid metal or semimetal preferably silicon
  • the temperature is increased within from 20 to 700 minutes to the temperature level required for pulling a single crystal, for example to the range of from 1300° C. to 1500° C.
  • a single crystal After the melting of the metal or semimetal, preferably polycrystalline silicon, a single crystal can be pulled by employing parameters known from the prior art.
  • the oxygen level in a crystal that has been pulled from a silica glass crucible produced using the method of the invention is higher than in a crystal that has been pulled from a conventional quartz crucible.
  • the density of oxygen precipitates in the single crystal after standard heat treatment (4 h 780° C., 16 h 1000° C.), however, is significantly lower than in crystals from conventional quartz crucibles.
  • the thick crystalline layer formed in the method according to the invention acts as a diffusion barrier for impurities that would otherwise enter the Si single crystal via the Si melt, and there act as seeds for the oxygen precipitates.
  • the process of the invention therefore makes it possible in a concerted process to produce a crucible with controlled levels of crystallization, followed by pulling a single crystal, preferably an Si single crystal pulled by means of a CZ method.
  • the invention thus also pertains to a method for pulling a single crystal from a melt of a metal or semimetal in a crucible, wherein a silica glass green body, which has been infiltrated with a substance that promotes crystallization, preferably cristobalite formation, is used as the crucible.
  • the invention further pertains to the use of a silica glass green body, which is infiltrated with a substance that promotes cristobalite formation, for pulling a single crystal, preferably an Si single crystal.
  • a thick crystalline crucible inner layer formed in the method of the invention offers the following advantages for simultaneously performed single-crystal pulling:
  • the growth rate of gas bubbles, which are present in the starting material, is significantly reduced in the crystalline region because of the higher viscosity of crystalline quartz compared with amorphous quartz glass.
  • the likelihood of the emission of quartz particles into the Si melt is significantly reduced by creating a crystalline inner layer that is more than 1 mm thick. This has a positive effect on dislocation-free crystal yield.
  • Reduction in the emission of quartz particles into the melt is due to the slower growth rate of the gas bubbles and the reduced mechanical stress at the inner surface of the crucible.
  • the mechanical stress is reduced, compared with known quartz glass crucibles with a thin crystalline inner layer, since the transition from the crystalline structure to the amorphous structure is shifted into the interior of the crucible wall.
  • crystalline layers can be used as a diffusion barrier to protect the Si melt against impurities.
  • the action of a crystalline surface layer as a diffusion barrier is shown by the reduced oxygen precipitation level in the single crystal (FIG. 3 ).
  • the reduced impurity level of the Si melt when employing such crucibles leads to a smaller number of seeds at which oxygen precipitates can form in the single crystal during the cooling phase.
  • the crystalline outer layer formed in the inventive method offers the several advantages for simultaneously performed single-crystal pulling.
  • a crystalline outer layer that is preferably at least 2 mm thick increases the mechanical stability of the crucible.
  • the thickness of the crystalline layer can be selected such that the crucible, although sintered in the melting phase of the CZ method, does not experience any change in its geometrical dimensions.
  • a crystalline layer formed in the inventive method and situated in the interior of the crucible wall also provides several advantages for simultaneously performed single-crystal pulling.
  • a crystalline layer situated in the interior of the silica glass crucible constitutes an effective diffusion barrier for impurity elements at the high temperatures prevailing in the pulling method (for example the CZ method), and it provides the opportunity to separate regions of the crucible that are manufactured using high-purity materials from those with lesser material quality.
  • the production costs for crucibles, in which the materials that enter into contact with liquid metal (for example Si) must meet the most stringent purity requirements, can thereby be reduced significantly.
  • a particular advantage when pulling single crystals is obtained by a silica glass crucible that is fully transformed into crystalline quartz during the heating phase of the CZ method.
  • the silica glass green body permeated homogeneously with the crystallization-inducing compound, is heated in the filled state to a temperature of 1300° C. within from 50 to 1500 minutes.
  • the temperature is increased to the temperature level required for pulling a single crystal, preferably to the range of from 1300° C. to 1500° C. Owing to the higher mechanical stability of such a crucible, the wall thickness can be reduced.
  • the crucibles can therefore be manufactured less expensively.
  • Increasing the stability of quartz glass crucibles by doping, for example with aluminum oxides, known from the literature may be avoided, as fully crystalized crucibles have a significantly lower impurity level for equal stability.
  • the mobility of the impurities that are present is significantly reduced by the lower diffusion constant in crystalline SiO 2 as compared with amorphous SiO 2 , which reduces the impurity level of the Si melt, and therefore also of the Si single crystal that is pulled.
  • the higher viscosity of crystalline SiO 2 also entails a reduction in the growth rate of gas bubbles that have been included in the material during the production process. This lowers the risk that displaced bubbles may emit quartz particles into the Si melt.
  • a fully crystalline crucible furthermore exhibits no corrosion phenomena on the inside of the crucible during contact with liquid Si. Mechanical stresses between crystalline and amorphous regions are furthermore avoided owing to the homogeneous material properties. Nevertheless, the opportunity to employ starting materials of different purity for the inner layer and the outer layer of the silica glass crucible still exists.
  • the structure of the crucible surface can be varied from closed and pore-free, preferably with a concentration of from 0.01 to 100 ⁇ g of compound per g of SiO 2 , to a very open-pored structure, preferably with a concentration of from 100 to 1000 ⁇ g of compound per g of SiO 2 .
  • the open-pored structure has a significantly larger surface area wetted with Si compared with the closed structure. This leads to an increase in the delivery of oxygen to the Si melt, and constitutes a suitable way of increasing the oxygen concentration of a crystal.
  • High-purity fumed and fused silica were dispersed homogeneously, without bubbles and without metal contamination, in double-distilled H 2 O under vacuum with the aid of a plastic-coated mixer.
  • the dispersion produced in this way had a solids content of 83.96% by weight (95% fused and 5% fumed silica).
  • the dispersion was shaped into a 14′′ crucible in a plastic-coated outer mold by means of the so-called roller method which enjoys widespread in the ceramic industry. After 1 hour of partial drying at a temperature of 80° C., the crucible could be released from the mold and dried to completion within 24 hours at about 200° C.
  • the dried open-pored silica glass green body had a density of approximately 1.62 g/cm 3 and a wall thickness of 9 mm.
  • the silica glass green body was uniformly sprayed on the inside and on the outside with 40 g of a 0.2% by weight strength aqueous BaOH solution.
  • an inner layer and an outer layer each with a layer thickness of 3 mm were infiltrated with barium hydroxide.
  • the barium concentration in these layers was in this case 46 ⁇ g per gram of SiO 2 .
  • the crucible was dried for 4 hours at 200° C.
  • the silica glass green body with a diameter of 14′′ from Example 1 was placed in a graphite support crucible customary for the CZ pulling of Si single crystals, and was filled with 28 kg of polycrystalline silicon.
  • the normally supplied electrical power for melting the silicon was modified so that a temperature of 1300° C. was reached within 80 minutes in the radial region of the silica glass green body. Under these conditions, transformation of the porous silica glass into cristobalite took place before liquid Si came into contact with the wall of the silica glass crucible.
  • the melting time is increased by 20% compared with the standard method.
  • a seed crystal After melting of the silicon, a seed crystal is immersed in the melt, and the crystal growth thereon begins.
  • the crystal pulling process takes place using conventional methodology, by producing a thin neck to eliminate undesired dislocations, subsequently increasing the diameter in the shoulder or cone region to the desired target diameter and continuing to produce a cylindrical single crystal.
  • an end cone is pulled at the end of the cylindrical part by reducing the diameter of the crystal to zero over a predetermined length.
  • the diameter in the cylindrical region of the single crystal was 129 mm. Both an inner and an outer 100% crystalline layer of cristobalite were created in the crucible walls during the pulling process (FIG. 1 ).
  • test wafers were taken from a plurality of positions along the axis of the cylindrical region, in order to determine the interstitial oxygen content (Oi) of the crystal by means of FTIR (Fourier Transformation Infrared Spectroscopy) according to the ASTM standard. Measurement results of single crystals, for whose production amorphous quartz glass crucibles were employed, are used as a comparison basis. The process parameters during the growth of the crystal were identical from the thin neck to the end cone for the crystal according to the process of subject invention Example 2 and the single crystals of the comparison group.
  • FTIR Fastier Transformation Infrared Spectroscopy
  • the interstitial oxygen content (Oi content) of the crucible produced according to the invention was 1.10 17 at/cm 3 higher than the Oi content of a conventional quartz crucible (see FIG. 2 ).

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Metallurgy (AREA)
  • Manufacturing & Machinery (AREA)
  • Ceramic Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Glass Melting And Manufacturing (AREA)
US10/292,059 2001-11-15 2002-11-12 Method for the production of a silica glass crucible with crystalline regions from a porous silica glass green body Expired - Fee Related US6946030B2 (en)

Applications Claiming Priority (2)

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DE10156137A DE10156137B4 (de) 2001-11-15 2001-11-15 Verfahren zur Herstellung eines Kieselglastiegels mit kristallinen Bereichen aus einem porösen Kieselglasgrünkörper
DEDE10156137.7 2001-11-15

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JP (1) JP2003146793A (fr)
KR (1) KR100512802B1 (fr)
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DE (1) DE10156137B4 (fr)
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US20040112274A1 (en) * 2002-10-09 2004-06-17 Japan Super Quartz Corporation Reinforcing process of silica glass substance and reinforced silica glass crucible
US20070007860A1 (en) * 2005-07-08 2007-01-11 Seiko Epson Corporation Actuator device, liquid-jet head and liquid-jet apparatus
US20090266110A1 (en) * 2006-09-29 2009-10-29 Heraeus Quarzglas Gmbh & Co. Kg SiO slurry for the production of quartz glass as well as the application of the slurry
KR200446667Y1 (ko) * 2008-12-29 2009-11-19 주식회사수성기술 솔라셀용 실리콘 잉곳 제조장치
US20110129784A1 (en) * 2009-11-30 2011-06-02 James Crawford Bange Low thermal expansion doped fused silica crucibles
TWI473771B (zh) * 2011-05-25 2015-02-21 Saint Gobain Res Shanghai Co Ltd 石英坩堝及其製造方法

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US7111476B2 (en) * 1994-06-30 2006-09-26 Ted A Loxley Electrophoretic deposition process for making quartz glass products
DE10260320B4 (de) * 2002-12-20 2006-03-30 Wacker Chemie Ag Verglaster SiO2-Formkörper, Verfahren zu seiner Herstellung und Vorrichtung
DE10319300B4 (de) * 2003-04-29 2006-03-30 Wacker Chemie Ag Verfahren zur Herstellung eines Formkörpers aus Kieselglas
DE102004003450A1 (de) * 2004-01-22 2005-08-18 Universität des Saarlandes Verfahren zur Herstellung dotierter oder undotierter Gläser aus Glaspulvern
DE102005032790A1 (de) * 2005-06-06 2006-12-07 Deutsche Solar Ag Behälter mit Beschichtung und Herstellungsverfahren
DE102005047112A1 (de) * 2005-09-30 2007-04-05 Wacker Chemie Ag In Teilbereichen oder vollständig verglaster amorpher SiO2-Formkörper, der bei höheren Temperaturen im verglasten Bereich kristallin wird, Verfahren zu seiner Herstellung und Verwendung
DE102007049634A1 (de) * 2007-10-17 2009-04-23 Technische Universität Bergakademie Freiberg Verfahren zur Erhöhung der Korrosionsbeständigkeit von Feuerfestmaterialien
CN102060553B (zh) * 2010-11-26 2013-01-09 上海交通大学 石英陶瓷坩埚的制备方法
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JP2003146793A (ja) 2003-05-21
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FR2832163A1 (fr) 2003-05-16
TW200300180A (en) 2003-05-16

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